CN113008721A - Rehmannia root moistening stop condition analysis method based on water content change - Google Patents

Rehmannia root moistening stop condition analysis method based on water content change Download PDF

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CN113008721A
CN113008721A CN202110198035.0A CN202110198035A CN113008721A CN 113008721 A CN113008721 A CN 113008721A CN 202110198035 A CN202110198035 A CN 202110198035A CN 113008721 A CN113008721 A CN 113008721A
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许鹏程
潘敏
徐广忠
易云建
丁国锦
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Anhui Xusong Traditional Chinese Medicine Pieces Co ltd
Bozhou Maixin Traditional Chinese Medicine Technology Co ltd
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Abstract

The invention provides a rehmannia root moistening stop condition analysis method based on water content change, which comprises the following specific steps of: raw material preparation, batch lubrication experiment, water absorption analysis, result analysis and verification experiment, wherein the water absorption analysis comprises the following steps: theoretical draft curve equation, parameter estimation and inflection point analysis, and the result analysis comprises the following steps: fitting a draft curve and calculating the moisture content; the rehmannia root wetting stop condition analysis method based on the water content change is reasonable in design, the fiber saturated water content is used as the basis, the wetting process stop condition of a wetting link in the processing process of the prepared rehmannia root is given, the saturated water content value of the prepared rehmannia root is obtained through experiments, the saturated water content is used as a stop node for wetting, the loss of the effective content of the prepared rehmannia root can be reduced better, a satisfactory color effect is obtained, the fiber saturated water content is used as a stop node for wetting the prepared rehmannia root, and the quality of the prepared rehmannia root can be better guaranteed.

Description

Rehmannia root moistening stop condition analysis method based on water content change
Technical Field
The invention belongs to the technical field of rehmannia root processing, and particularly relates to a rehmannia root moistening stop condition analysis method based on water content change.
Background
The surface of dried rehmannia root is gray black or brown-gray, the section is black, brown-black or black. After steaming, the color of the rehmannia becomes black paint, mainly because Maillard reaction occurs in the rehmannia[4]. The maillard reaction is also called "non-enzymatic browning reaction", which is a kind of non-enzymatic browning reaction widely existing in food industry, is a reaction between carbonyl compounds (reducing saccharides) and amino compounds (amino acids and proteins), and finally generates a brown or even black macromolecular substance melanoidin or melanomimetic through a complicated process, so the maillard reaction is also called as a carbonylamino reaction. The maillard reaction is strongly related to the water molecule activity in the article. Studies have shown that maillard reactions occur most readily when the water activity is between 0.6 and 0.7, and that non-enzymatic browning increases with increasing water activity when the water is within a certain range. The water activity was reduced to 0.2 or less, and browning was difficult to progress. Water activity is greater than the high peak of browning and the speed is slowed down by the dilution of the solute. Both too high and too low water content are detrimental to the maillard reaction. Therefore, the control of the moisture content during the moistening process has an important influence on the color change during the steaming process of the prepared rehmannia root.
Generally, water exists in plants in three forms: bound water, attached water and free water. The bound water is the water in organic compounds in rehmannia glutinosa, exists in the form of ions and is difficult to evaporate. The attached water adheres to the cell wall and exists in the form of molecules, without fluidity. The air-drying at normal temperature can not volatilize the volatile matter. Free water is present in the tube space between cells and has fluidity. The air-drying at normal temperature can evaporate the water. When the plant has only attached water and no free water, the plant is said to have reached its fiber saturation water content, also known as saturated water content. In order to reduce the content of effective substances in rehmannia glutinosa Libosch, especially the extract content, the content of free water should be minimized.
Therefore, the moistening process of the prepared rehmannia root processing is an important link. If the moistening time is too short and the water content of rehmannia root is not in the optimum requirement of Maillard reaction, the steaming time needs to be prolonged. When the water content is too high, the rate of Maillard reaction is reduced because the solute is diluted, the steaming time is required to be added, and the loss of verbascoside is increased because of too long steaming time. Meanwhile, if the moistening time is too long, the content of free water in the rehmannia root is too high, which causes the loss of water-soluble substances and influences the quality of the prepared rehmannia root decoction pieces. However, in the existing processing technology of the prepared rehmannia root, the moistening process mainly depends on experience, and an executable stopping condition is not provided. Although researches on moisture content change and water activity change in the traditional Chinese medicine processing process are paid attention by researchers, the key problems to be solved in the moistening link are how to find the optimal moisture content for the optimal moistening and how to control the moisture content change in the moistening process, and therefore, the invention provides a rehmannia root moistening stop condition analysis method based on the moisture content change.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a rehmannia root moistening stop condition analysis method based on water content change, the rehmannia root wetting stop condition analysis method based on the water content change has reasonable design, gives the stop condition of the wetting process in the wetting link in the processing process of the prepared rehmannia root based on the fiber saturated water content, the saturated water content value of the radix rehmanniae recen is obtained through experiments, the saturated water content is used as a stop node for infiltration, the loss of the effective content of the radix rehmanniae recen can be better reduced, and obtains satisfactory color effect, and the fiber saturated water content is used as the infiltration stop node of the processing of the prepared rehmannia root, the quality of the prepared rehmannia root can be better ensured, meanwhile, the research on the saturated water content of the prepared rehmannia root by the weighing method also provides a simple and feasible thought for the research on the saturated water content of the prepared rehmannia root, and the method has very important guiding significance in the processing of the prepared rehmannia root.
In order to achieve the purpose, the invention is realized by the following technical scheme: a rehmannia root lubrication stop condition analysis method based on water content change comprises the following specific steps:
the method comprises the following steps: preparing raw materials; selecting proper rehmannia as an experimental raw material according to needs, and inspecting the experimental raw material;
step two: performing batch lubrication experiment; the preparation experiment is divided into 16 batches, each batch is 1.5kg, according to the stipulation of pharmacopeia, firstly, impurities of rehmannia root raw medicinal materials are removed, the rehmannia root raw medicinal materials are cleaned, the cleaned rehmannia root is put into a plastic turnover basket and placed in a water bath box or a thermostat with set temperature, in each experiment batch, the total weight of the materials is weighed after 2h, 5 representative samples are taken out, the weight is accurately weighed by a high-precision balance, then the weight of 5 representative samples is weighed by the high-precision balance before each soaking, 80 groups of sample data are obtained, each group has 12 data, and the change process of the water content of the rehmannia root in the whole moistening process is calculated according to the change of the weight in the moistening process recorded by the data;
step three: analyzing the absorbed water; the method comprises the following specific steps:
theoretical draft curve equation: the water absorption process of the rehmannia is a diffusion equation, according to the appearance characteristics of the rehmannia, the rehmannia is assumed to be a standard cylinder, so that the water absorption process of the rehmannia can be described by applying a cylindrical coordinate diffusion equation, and the transverse change of the water in the rehmannia is ignored, so that the water absorption process of the rehmannia can be expressed by using a one-dimensional cylindrical coordinate diffusion equation:
(1)
wherein w (t, r) is a water content distribution function inside the rehmannia root, r is the radius of the cylinder, namely the average radius of the rehmannia root, and in order to simplify the model, the water is considered to be uniformly distributed inside the rehmannia root, so that the water content change process of the rehmannia root can be analyzed by using a lumped heat capacity method, and the equation is as follows:
(2)
wherein W (t) is the water content in rehmannia root, WbWater content of surface of rehmannia glutinosa Libosch, W0Is the initial water content of rehmannia, and H is the intersection between the object and the surrounding fluidIn terms of conversion coefficient, C is the volume coefficient of the object, V is the volume, a is the surface area, ρ is the density of the object, and equation (2) can be written as:
W=Wb+(W0-Wb)(3)
let β be hA/(ρ VC), the above equation can be written as:
W(t)=Wm(1-exp(-β(t+t0))(4)
in the equation, WmCalled maximum water content (saturated water content), is the value of the maximum water content that can be achieved inside rehmannia glutinosa, beta is the water absorption coefficient of rehmannia glutinosa, the size of which is related to the radius of rehmannia glutinosa, and t is0The time offset is related to the initial water content of the rehmannia root, and the equation is called as an immersion water content change equation;
estimating parameters: based on the weight observation and the laboratory test results, observed values of water content of the rehmanniae radix sample at 13 times can be obtained, and the observed values are recorded as (t)n,wn) These data are substituted into equation (4) and the parameter values of equation (4) are estimated using the least squares method, taking into account the minimum of the following functions:
F(Wn,β,t0)=∑n||Wn-Wm(1-exp(-β(tn-t0))||2
because the least squares equation is non-linear, a Levenberg-Marquard algorithm is applied to estimate the parameter values, the specific algorithm is as follows:
(1): selecting an initial point
Figure BDA0002946723580000051
Termination control constant ε 10-5Calculating epsilon0=||Wn-W(tn)||,k=0;γ0=10-3,v=10;
(2): calculating the Jacobian matrix J of the function w (t)kConstructing an incremental equation:
Figure BDA0002946723580000052
(3): solving the incremental equation to obtain deltakIf W-F (p)kk)||<εkLet p stand fork+1=pkkIf | | | δkIf | < epsilon, stopping iteration, otherwise, gammak+1=γkV, returning to the step (2);
(4): if | | | W-F (p)kk)||≥εk,γk+1=vγkCalculating deltakReturning to the step (1);
analysis of inflection points: according to the characteristics of the exponential function, when 1 ≦ exp (x) ≦ 0.35, the exponential function is closer to a straight line, (R)2Greater than 0.98), and therefore, 0.35 for exp (x) is said to be the inflection point of the curve, before which the exponential function approaches a straight line, and 0.35. ltoreq. exp (x) 0.15 for which the curve of the exponential function approaches a quadratic function, and therefore W is said to ber=0.65WmThe moistening water content of rehmannia;
step four: analyzing results; the method comprises the following specific steps:
fitting of a draft curve: weighing according to the initial water content and the weight to obtain the value of the water content of the rehmannia every 2 hours, and obtaining a fitting result of a draft curve by applying a nonlinear least square method;
calculating the content of the moistening water: according to the simulation result of the water content of the rehmannia root, the maximum water content and the value of the moistening water content of the rehmannia root can be obtained at different moistening temperatures;
step five: verifying the experiment; performing two-batch verification with appropriate rehmanniae radix, dividing each batch into 4 groups, each group containing 1.4kg, moistening for 4h, 7h, 10h and 13h, steaming for 3h (100 deg.C), oven drying, slicing, oven drying to water content of about 13%, and inspecting in laboratory to obtain effective content of radix rehmanniae Preparata decoction pieces, extract content and radix rehmanniae Preparata appearance score.
In a preferred embodiment of the present invention, in the first step, the items to be checked include: water, extract, verbascoside and total ash.
As a preferred embodiment of the present invention, the production area and quality of the rehmannia root of different batches in the step five are the same.
In a preferred embodiment of the present invention, the cleaning process in the second step is not more than 5 min.
In a preferred embodiment of the present invention, in the fourth step (i), the initial water content is a laboratory water content detection result.
The invention has the beneficial effects that:
1. the rehmannia root wetting stop condition analysis method based on the water content change provides the wetting process stop condition of the wetting link in the processing process of the prepared rehmannia root based on the fiber saturated water content, the saturated water content value of the radix rehmanniae recen is obtained through experiments, and the value is applied to carry out the verification experiment of the processing of the radix rehmanniae preparata, and the verification experiment shows that the saturated water content is used as the stop node of infiltration, the loss of the effective content of the radix rehmanniae recen can be better reduced, and obtains satisfactory color effect, experiments prove that the quality of the prepared rehmannia root can be better ensured by taking the fiber saturated water content as an infiltration stop node for the processing of the prepared rehmannia root, meanwhile, the research on the saturated water content of the prepared rehmannia root by the weighing method also provides a simple and easy thought for the research on the saturated water content of the prepared rehmannia root, and the method and the conclusion have very important guiding significance in the processing of the prepared rehmannia root.
2. According to the rehmannia root moistening stop condition analysis method based on the change of the water content, the change curve of the water content of rehmannia root in the moistening process is obtained by observing the change of the water content of rehmannia root and applying a diffusion equation to obtain a water content change equation of the rehmannia root, the water content value of the rehmannia root at the moment when the rehmannia root is saturated with adsorbed water and free water is little is obtained by analyzing the inflection point of the curve, the water content value is called as a moistening water content value, the moistening water content value is used as a stop condition of the moistening process in the rehmannia root processing, the stop condition can well guarantee the steaming effect of the rehmannia root and the maintenance of effective components through comparative experiment analysis, a clear stop condition is provided for the moistening process in the rehmannia root processing process, and theoretical support is provided for the development of a linkage line and an automatic line process of the prepared rehmannia root.
Drawings
FIG. 1 is a flow chart of a method for analyzing conditions for stopping moistening rehmanniae based on changes in water content according to the present invention.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Referring to fig. 1, the present invention provides a technical solution: a rehmannia root lubrication stop condition analysis method based on water content change comprises the following specific steps:
the method comprises the following steps: preparing raw materials; selecting proper rehmannia as an experimental raw material according to needs, and inspecting the experimental raw material, wherein rehmannia produced in Henan Wu 38495county 2015 and 2017 is used as the experimental raw material, and the inspection results of the raw material are as follows:
table 1 raw material test results
Figure BDA0002946723580000081
Step two: performing batch lubrication experiment; the experiment is divided into 16 batches, each batch is 1.5kg, according to the regulation of pharmacopeia, firstly removing impurities from the raw rehmannia root, cleaning, loading the cleaned rehmannia root into a plastic turnover basket, and placing the plastic turnover basket in a water bath box or a thermostat with a set temperature, wherein the experimental environment of the 16 batches is summarized as follows:
TABLE 2 Experimental batch temperature and humidity setting table
Figure BDA0002946723580000091
Weighing the total weight of the materials after 2 hours in each experimental batch, taking out 5 representative samples, accurately weighing the weight by using a high-precision balance, weighing the weight of the 5 representative samples by using the high-precision balance before soaking each time to obtain 80 groups of sample data, wherein each group contains 12 data, and calculating the change process of the water content of the rehmannia in the whole moistening process according to the change of the weight of the rehmannia in the moistening process recorded by the data;
step three: analyzing the absorbed water; the method comprises the following specific steps:
theoretical draft curve equation: the water absorption process of the rehmannia is a diffusion equation, according to the appearance characteristics of the rehmannia, the rehmannia is assumed to be a standard cylinder, so that the water absorption process of the rehmannia can be described by applying a cylindrical coordinate diffusion equation, and the transverse change of the water in the rehmannia is ignored, so that the water absorption process of the rehmannia can be expressed by using a one-dimensional cylindrical coordinate diffusion equation:
(1)
wherein w (t, r) is a water content distribution function inside the rehmannia root, r is the radius of the cylinder, namely the average radius of the rehmannia root, and in order to simplify the model, the water is considered to be uniformly distributed inside the rehmannia root, so that the water content change process of the rehmannia root can be analyzed by using a lumped heat capacity method, and the equation is as follows:
(2)
wherein W (t) is the water content in rehmannia root, WbWater content of surface of rehmannia glutinosa Libosch, W0For the initial water content of rehmannia, H is the exchange coefficient between the object and the surrounding fluid, C is the volume coefficient of the object, V is the volume, A is the surface area, ρ is the density of the object, and equation (2) can be written as:
W=Wb+(W0-Wb)(3)
let β be hA/(ρ VC), the above equation can be written as:
W(t)=Wm(1-exp(-β(t+t0))(4)
in the equation, WmCalled maximum water content (saturated water content), is the value of the maximum water content that can be achieved inside rehmannia glutinosa, beta is the water absorption coefficient of rehmannia glutinosa, the size of which is related to the radius of rehmannia glutinosa, and t is0The time offset is related to the initial water content of the rehmannia root, and the equation is called as an immersion water content change equation;
estimating parameters: based on the weight observation and the laboratory test results, observed values of water content of the rehmanniae radix sample at 13 times can be obtained, and the observed values are recorded as (t)n,wn) These data are substituted into the formula (4), and the parameters of the formula (4) are estimated by applying the least square methodNumerical values, i.e. taking into account the minimum of the following function:
F(Wn,β,t0)=∑n||Wn-Wm(1-exp(-β(tn-t0))||2
because the least squares equation is non-linear, a Levenberg-Marquard algorithm is applied to estimate the parameter values, the specific algorithm is as follows:
(1): selecting an initial point
Figure BDA0002946723580000111
Termination control constant ε 10-5Calculating epsilon0=||Wn-W(tn)||,k=0;γ0=10-3,v=10;
(2): calculating the Jacobian matrix J of the function w (t)kConstructing an incremental equation:
Figure BDA0002946723580000121
(3): solving the incremental equation to obtain deltakIf W-F (p)kk)||<εkLet p stand fork+1=pkkIf | | | δkIf | < epsilon, stopping iteration, otherwise, gammak+1Returning to the step (2) when the ratio is gamma k/v;
(4): if | | | W-F (p)kk)||≥εk,γk+1=vγkTo find epsilonkReturning to the step (1);
analysis of inflection points: according to the idea of wood drying, the water inside plant cells can be divided into three types, namely, bound water, adsorbed water and free water, wherein the bound water is the water in compounds inside the cells, the part of water is not easy to evaporate, the adsorbed water is the water inside the cells and in cell walls, the free water is intercellular space water, rehmannia absorbs the water and firstly enters the cells to become adsorbed water, the water absorption speed of the cells is high, when the water inside the cells is saturated, the water absorbed by the rehmannia is mainly filled in the intercellular spaces to become free water, the mobility of the water is high, the water absorption speed of the rehmannia is slow, when the adsorbed water is saturated and the free water is not present, the wood is called fiber saturated water, in the research of wood and traditional Chinese medicine, the method for detecting the water activity or the saturated water content is various, including a physical characteristic method and a calorimeter scanning method, nuclear magnetic resonance method, solute extension method, but these methods depend on the apparatus with high requirements, unsuitable for the production needs, because the speed of absorbing and adsorbing water and free water of the cell is different, the study shows, in the course of absorbing water, the speed of absorbing and adsorbing water of the plant is faster, and the speed of absorbing and adsorbing free water becomes slower, the speed of absorbing and adsorbing water is generally constant, and is a quadratic function when absorbing free water, there is the property that researchers apply, search for the value of the saturated water content in the drying process of the timber, get good results, this paper is using this method to detect the value of the saturated water content in the infiltration process of the rehmannia glutinosa libosch;
according to the characteristics of the exponential function, when 1 ≦ exp (x) ≦ 0.35, the exponential function is closer to a straight line, (R)2Greater than 0.98), and therefore, 0.35 for exp (x) is said to be the inflection point of the curve, before which the exponential function approaches a straight line, and 0.35. ltoreq. exp (x) 0.15 for which the curve of the exponential function approaches a quadratic function, and therefore W is said to ber=0.65WmThe moistening water content of rehmannia;
step four: analyzing results; the method comprises the following specific steps:
fitting of a draft curve: weighing according to the initial water content and the weight to obtain a value of the water content of the rehmannia every 2 hours, obtaining a fitting result of a draft curve by applying a nonlinear least square method, wherein the fitting result of the water content observation value and the water content change curve can show that the given water diffusion model can well describe the process of the water change in the rehmannia, so that the feasibility of finding an inflection point of the water content change curve and finding the moisture content is provided;
TABLE 3 straight-line fitting results of exponential function
Figure BDA0002946723580000141
Calculating the content of the moistening water: according to the simulation results of the water content of rehmannia, the maximum water content and the moistening water content of rehmannia at different moistening temperatures can be obtained, for example, the estimated values of HN1502 are shown in the following table:
TABLE 4 HN502 maximum Water content and Permeability Water content
Figure BDA0002946723580000142
As a result, the relationship between the moistening water content and the temperature is relatively large, the temperature is increased, the moistening time and the moistening water content are reduced, the water activity in the rehmannia root is increased due to the increased temperature, the saturation point of the absorbed water is reduced, the moistening water content and the moistening time are reduced, and the relationship between the moistening water content and the moistening time and the temperature is as follows:
Figure BDA0002946723580000143
Figure BDA0002946723580000151
the results show that the moisture content of the rehmannia glutinosa is in a range of 20-35%, the moisture content is reduced along with the increase of the temperature, the reaching time of the moisture content is reduced along with the increase of the temperature, the basic reaching time is in a range of 8-20h, but the batch difference is obvious;
step five: verifying the experiment; performing two-batch verification by using rehmannia glutinosa Libosch produced in Henan, wherein each batch is divided into 4 groups, each group is 1.4kg, the materials are moistened according to four time periods of 4h, 7h, 10h and 13h, finally the materials are uniformly steamed for 3h (100 ℃), dried and sliced, the decoction pieces are dried until the water content is about 13%, and a sample is sent to a laboratory for inspection to obtain the effective content value of the prepared rehmannia root decoction pieces, the content value of extract and the appearance score of the prepared rehmannia root;
in the experiment, a 6-disc steaming cabinet, a GZX-9146MBE hot air blast drying oven and a DHG-9140A type electric heating constant temperature blast drying oven are used for carrying out the inspection according to the requirements of pharmacopeia (chromatograph: thermal ultimate3000), and the inspection results are as follows:
table 5 validated Water content results
Figure BDA0002946723580000152
Table 6 shows the results of the test
Figure BDA0002946723580000153
Figure BDA0002946723580000161
In the validation experiment, the water content of the infiltration batch with the longest infiltration time (see table 5) was calculated, and the water penetration content of the validation batch was 32.15; the moistening time is 9.38 hours, the prepared rehmannia is obtained by steaming for 3 hours, through observing the appearance and the interior of the prepared rehmannia, the prepared rehmannia is steamed after being moistened for 4 hours and 7 hours, the appearance effect is obviously inferior to that of the moistened rehmannia for 10 hours and 13 hours, the prepared rehmannia is locally yellow and moistened for 4 hours and 7 hours, the interior of the steamed prepared rehmannia is dry, although the color of the prepared rehmannia also reaches black like paint, the prepared rehmannia is obviously not moistened enough, and the moistening effect of the prepared rehmannia in 10 hours and 13 hours is obviously improved, the result can also be seen that the optimal moistening time of the prepared rehmannia is about 10 hours, which is consistent with the theoretical result;
meanwhile, the rehmannia root test results (Table 6) show that the extract content of the verified batch is not changed greatly, the extract content of 13h infiltrated samples of the verified batch is slightly reduced, the content detection of verbascoside shows that samples infiltrated for 13h are obviously reduced compared with samples infiltrated for 10h, which shows that the infiltration time is overlong and has obvious loss on the content of verbascoside, which also proves that the saturated water content is the optimal infiltration stop node in the processing of prepared rehmannia root, the fiber saturated water content is taken as the basis, the infiltration process stop condition of the infiltration link in the processing process of the prepared rehmannia root is given, the saturated water content value of the prepared rehmannia root is obtained through experiments, and the verification experiments of the processing of the prepared rehmannia root are carried out by applying the value, and the verification experiments show that the loss of the effective content of the prepared rehmannia root can be better reduced by applying the saturated water content as the infiltration stop node, experiments prove that the quality of the prepared rehmannia root can be better ensured by taking the fiber saturated water content as an infiltration stop node for processing the prepared rehmannia root, and meanwhile, a simple and easy thought is provided for the research on the saturated water content of the prepared rehmannia root by a weighing method;
in a preferred embodiment of the present invention, in the first step, the items to be checked include: water, extract, verbascoside and total ash.
As a preferred embodiment of the present invention, the production area and quality of the rehmannia root of different batches in the step five are the same.
In a preferred embodiment of the present invention, the cleaning process in the second step is not more than 5 min.
In a preferred embodiment of the present invention, in the fourth step (i), the initial water content is a laboratory water content detection result.
While there have been shown and described what are at present considered the fundamental principles and essential features of the invention and its advantages, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (5)

1. A rehmannia root lubrication stop condition analysis method based on water content change is characterized by comprising the following specific steps:
the method comprises the following steps: preparing raw materials; inspecting the raw materials according to the diameter of the rehmannia;
step two: weighing the weight and calculating the water content in the moistening process; wetting sorted rehmannia, according to the specification of pharmacopoeia, firstly removing impurities from raw rehmannia materials, cleaning, putting the cleaned rehmannia root into a plastic turnover basket, placing the plastic turnover basket in a water bath box or a thermostat with a set temperature, weighing the total weight of the materials after 2 hours in each experimental batch, and calculating the change process of the water content of the rehmannia root in the whole wetting process according to the change of the weight of the rehmannia root recorded by the data in the wetting process; the initial water content of rehmanniae radix is w0The initial weight of rehmannia is H0The weight of rehmannia root in the moistening process is HiThe water content of rehmanniae radix in the moistening process is
Figure FDA0002946723570000011
Step three: water absorption curve analysis and estimation:
theoretical draft curve equation: the water absorption process of the rehmannia is a diffusion equation, according to the appearance characteristics of the rehmannia, the rehmannia is assumed to be a standard cylinder, so that the water absorption process of the rehmannia can be described by applying a cylindrical coordinate diffusion equation, and the transverse change of the water in the rehmannia is ignored, so that the water absorption process of the rehmannia can be expressed by using a one-dimensional cylindrical coordinate diffusion equation:
(1)
wherein w (t, r) is a water content distribution function inside the rehmannia root, r is the radius of the cylinder, namely the average radius of the rehmannia root, and in order to simplify the model, the water is considered to be uniformly distributed inside the rehmannia root, so that the water content change process of the rehmannia root can be analyzed by using a lumped heat capacity method, and the equation is as follows:
(2)
wherein W (t) is the water content in rehmannia root, WbWater content of surface of rehmannia glutinosa Libosch, W0For the initial water content of rehmannia, H is the exchange coefficient between the object and the surrounding fluid, C is the volume coefficient of the object, V is the volume, A is the surface area, ρ is the density of the object, and equation (2) can be written as:
W=Wb+(W0-Wb)
(3)
let β be hA/(ρ VC), the above equation can be written as:
W(t)=Wm(1-exp(-β(t+t0))
(4)
in the equation, WmCalled maximum water content (saturated water content), is the value of the maximum water content that can be achieved inside rehmannia glutinosa, beta is the water absorption coefficient of rehmannia glutinosa, the size of which is related to the radius of rehmannia glutinosa, and t is0The time offset is related to the initial water content of the rehmannia root, and the equation is called as an immersion water content change equation;
estimating parameters: based on the weight observation and the laboratory test results, observed values of water content of the rehmanniae radix sample at 13 times can be obtained, and the observed values are recorded as (t)n,wn) These data are substituted into equation (4) and the parameter values of equation (4) are estimated using the least squares method, taking into account the minimum of the following functions:
Figure FDA0002946723570000031
because the least squares equation is non-linear, a Levenberg-Marquard algorithm is applied to estimate the parameter values, the specific algorithm is as follows:
(1): selecting an initial point
Figure FDA0002946723570000032
Termination control constant ε 10-5Calculating epsilon0=||Wn-W(tn)||,k=0;γ0=10-3,v=10;
(2): calculating the Jacobian matrix J of the function w (t)kConstructing an incremental equation:
Figure FDA0002946723570000033
(3): solving the incremental equation to obtain epsilonkIf W-F (p)kk)||<εkLet p stand fork+1=PkkIf | | | δkIf | < epsilon, stopping iteration, otherwise, gammak+1=γkV, returning to the step (2);
(4): if | | | W-F (p)kk)||≥εk,γk+1=vγkCalculating deltakReturning to the step (1);
step four: fiber saturation point and wet stop condition analysis:
fiber saturation point: generally, water exists in plants in three forms: bound water, attached water and free water. The bound water is the water in organic compounds in rehmannia glutinosa, exists in the form of ions and is difficult to evaporate. The attached water adheres to the cell wall and exists in the form of molecules, without fluidity. The air-drying at normal temperature can not volatilize the volatile matter. Free water is present in the tube space between cells and has fluidity. The air-drying at normal temperature can evaporate the water. When the plant has only attached water and no free water, the plant is said to have reached its fiber saturation water content, also known as saturated water content. The speed of the plant absorbing the attached water is high, and the change of the water content is linear; when the plant absorbs free water, the absorption speed becomes slow, and the change of the water content is a quadratic curve. According to the characteristic, the position of the fiber saturation point can be judged.
Judging inflection points (judging fiber saturation points): according to the characteristics of the exponential function, when 1. ltoreq. exp (x) 0.35, the exponential function is closer to oneStraight line, (R)2Greater than 0.98), so the term exp (x) 0.35 is the inflection point of the curve before which the exponential function approaches a straight line, and when 0.35. ltoreq. exp (x) 0.15 the curve of the exponential function approaches a quadratic function, so the term: wr=0.65WmIs the moisture content (fiber saturation point) of rehmannia;
③ determining a stopping condition: based on the characteristics of the fiber saturation point, we determined
1-exp(-β(t+t0)=0.65
Figure FDA0002946723570000051
The conditions for stopping the wetting were as follows.
Step five: verifying the experiment; performing two-batch verification with appropriate rehmanniae radix, dividing each batch into 4 groups, each group containing 1.4kg, moistening for 4h, 7h, 10h and 13h, steaming for 3h (100 deg.C), oven drying, slicing, oven drying to water content of about 13%, and inspecting in laboratory to obtain effective content of radix rehmanniae Preparata decoction pieces, extract content and radix rehmanniae Preparata appearance score.
2. A method for analyzing a condition for stopping moistening of rehmannia glutinosa based on a change in water content according to claim 1, wherein: in the first step, the items to be checked include: water, extract, verbascoside and total ash.
3. A method for analyzing a condition for stopping moistening of rehmannia glutinosa based on a change in water content according to claim 1, wherein: in the fifth step, the producing areas and the quality of the rehmannia roots of different batches are the same.
4. A method for analyzing a condition for stopping moistening of rehmannia glutinosa based on a change in water content according to claim 1, wherein: and the cleaning process in the second step is not more than 5 min.
5. A method for analyzing a condition for stopping moistening of rehmannia glutinosa based on a change in water content according to claim 1, wherein: in the fourth step, the initial water content is a laboratory water content detection result.
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CN113533315A (en) * 2021-07-06 2021-10-22 山东中医药大学 Method for evaluating processing quality of rehmannia by microscopic imaging technology

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113533315A (en) * 2021-07-06 2021-10-22 山东中医药大学 Method for evaluating processing quality of rehmannia by microscopic imaging technology

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